Production of metallic titanium



United PRODUCTION OF METALLIC TITANIUM No Drawing. Application April 12,1948, Serial No. 20,594

2 Claims. (Cl. 117-107) This invention relates to the production ofmetallic titanium and has for an object the provision of an improvedmethod or process for producing high-purity metallic titanium. Moreparticularly, the invention contemplates the provision of an improvedmethod or process for producing high-purity metallic titanium bydissociation of titanium tetraiodide.

According to some heretofore customary procedures, metallic titanium ofhigh purity is produced by contacting titanium tetraiodide with a heatedsurface maintained at a temperature in the range 1100 C. to 1700 C.Contact of the titanium tetraiodide with the heated surface results indissociation of the iodine and titanium of the titanium tetraiodide withdeposition of the titanium on the heated surface and with the productionof a gaseous product containing the iodine in vapor form. Titanium ortungsten or some other suitable metal is employed in forming the heatedsurface.

The titanium tetraiodide employed is formed by contacting iodine invapor form with crude metallic titanium. The dissociation operation iscarried out in a closed vessel or chamber under high vacuum, and theamount of titamum contained 1n each unit of volume of the vessel orchamber, and, consequently, the amount of titanium available fordeposition from each .unit of titanium tetraiodide vapor therein, isrelatively small.

The present invention provides a method of increasing the eificiency ofthe deposition operation by making available for deposition a greateramount of titanium is each unit of volume of the deposition vessel orcham- The invention utilizes that property of titanium triiodide whichpermits it to remain stable at elevated temperatures in the presence oftitanium tetraiodide, and, in utilizing that property, the inventionemploys, in the deposition vessel or chamber a mixture of titaniumtriiodide and titanium tetraiodide instead of titanium tetraiodidealone.

When the mixture of iodides contacts the heated surface, the tetraiodideis dissociated, disturbing the equilibrlum and permitting progressivedissociation of the triiodide in accordance with the followingequations:

In a preferred process of the invention, iodine in vapor form 1scontacted with titanium carbide at an elevated temperature such, forexample, as 1100 C., to produce a gaseous product comprising titaniumtetraiodide, the resulting gaseous product is contacted with crudetitanium metal such as scrap metal at a temperature in the range 600 C.to 1000 C. to produce a stable mixture of titates Patent 2,694,652Patented Nov. 16, 1954 'ice tanium tetraiodide and titanium triiodide,and the miX- ture is contacted with a heated surface at a temperature inthe range 1100 C. to 1700 C. to produce metallic titanium and a gaseousproduct containing elemental iodine.

The gaseous products containing elemental iodine are utilized in theproduction of additional titanium iodides. A gaseous product comprisingelemental iodine preferably is contacted with titanium carbide at atemperature of about 1100 C. to form a gaseous product containingtitanium tetraiodide which is contacted with metallic titanium at atemperature in the range 600 C. to 1000 C. to convert a portion of thetitanium tetraiodide to titanium triiodide to regenerate the gaseousproduct containing titanium tetraiodide and titanium triiodide forre-use in the deposition operation.

I claim:

1. The method of recovering titanium in the form of a high-puritymetallic product from crude titanium-bearing material which comprisescontacting a gaseous product comprising titanium tetraiodide andtitanium triiodide with a heater refractory surface maintained at atemperature in the range 1100 C. to 1700 C. to effect dissociation ofthe titanium tetraiodide and the titanium triiodide with the productionand deposition of metallic titanium on the refractory surface and theproduction of a gaseous product comprising elemental iodine, reactingthe elemental iodine thus produced with titanium carbide at atemperature of about 1100 C. to form a. gaseous product containingtitanium tetraiodide, reacting the titanium tetraiodide thus producedwith metallic titanium at a temperature in the range 600 C. to 1100 C.to convert a portion of the titanium tetraiodide to titanium triiodide,and passing the regenerated titanium tetraiodide and titanium triiodidein contact with the refractory surface for the production and depositionof additional metallic titanium.

2. The method of recovering titanium in the form of a high-puritymetallic product from crude titanium-bearing material which comprisescontacting a gaseous product comprising titanium tetraiodide andtitanium triiodide with a heated body of metallic titanium maintained ata temperature in the range 1100 C. to 1700 C. to eflect dissociation ofthe titanium tetraiodide and the titanium triiodide with the productionand deposition of metallic titanium on the body of metallic titanium andthe production of a gaseous product comprising elemental iodine,reacting the elemental iodine thus produced with titanium carbide at atemperature of about 1100 C. to form a gaseous product containingtitanium tetraiodide, reacting the titanium tetraiodide thus producedwith a crude titanium-bearing material at a temperature in the the range600 C. to 1100 C. to convert a portion of the titanium tetraiodide totitanium triiodide, and passing the regenerated titanium tetraiodide andtitanium tri iodide in contact with the heated body of metallic titaniumfor the production and deposition of additional quantities of metallictitanium.

References Cited in the file of this patent UNITED STATES PATENTS NumberName Date 1,497,417 Weber June 10, 1924 1,671,213 Van Arkel et a1 May29, 1928 1,891,124 Van Arkel et al Dec. 13, 1932 2,393,264 Rentschler eta1. Jan. 22, 1946 2,519,385 Loonam Aug. 22, 1950

1. THE METHOD OF RECOVERING TITANIUM IN THE FORM OF A HIGH-PURITYMETALLIC PRODUCT FROM CRUDE TITANIUM-BEARING MATERIAL WHICH COMPRISESCONTACTING A GASEOUS PRODUCT COMPRISING TITANIUM TETRAIODIDE ANDTITANIUM TRIIODIDE WITH A HEATER REFRACTORY SURFACE MAINTAINED AT ATEMPERATURE IN THE RANGE 1100* C. TO 1700* C. TO EFFECT DISSOCIATION OFTHE TITANIUM TETRAIODIDE AND THE TITANIUM TRIIODIDE WITH THE PRODUCTIONAND DEPOSITION OF METALLIC TITANIUM ON THE REFRACTORY SURFACE AND THEPRODUCTION OF A GASEOUS PRODUCT COMPRISING ELEMENTAL IODINE, REACTINGTHE ELEMENTAL IODINE THUS PRODUCED WITH TITANIUM CARBIDE AT ATEMPERATURE OF ABOUT 1100* C. TO FORM A GASEOUS PRODUCT CONTAININGTITANIUM TETRAIODIDE, REACTING THE TITANIUM TETRAIODIDE THUS PRODUCEDWITH METALLIC TITANIUM AT A TEMPERATUR IN THE RANGE 600* C. TO 1100* C.TO CONVERT A PORTION OF THE TITANIUM TETRAIODIDE TO TITANIUM TRIIODIDE,AND PASSING THE REGENERATED TITANIUM TETRAIODIDE AND TITANIUM TRIIODIDEIN CONTACT WITH THE REFRACTORY SURFACE OF THE PRODUCTION AND DEPOSITIONOF ADDITIONAL METALLIC TITANIUM.